CN101817806A - Method for preparing atractylon - Google Patents
Method for preparing atractylon Download PDFInfo
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- CN101817806A CN101817806A CN201010170570A CN201010170570A CN101817806A CN 101817806 A CN101817806 A CN 101817806A CN 201010170570 A CN201010170570 A CN 201010170570A CN 201010170570 A CN201010170570 A CN 201010170570A CN 101817806 A CN101817806 A CN 101817806A
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- distillation
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- atractylone
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing atractylon, which has the characteristic of simple and convenient operation, light pollution and low energy consumption. The method comprises the following process steps of: selecting a dry rhizome of plants, such as atractylis lancea, atractylodes chinensis and rhizoma atractylodis macrocephalae, crushing the rhizome, and adding the rhizome into a CO2 super critical extractor for extracting to obtain an extract; injecting the extract into a molecular distillation apparatus, and then performing two-grade molecular distillation on the extract in the molecular distillation apparatus, wherein the temperature of an evaporating surface of a first grade distillation is between 60 and 90 DEG C, the pressure is 100 to 150Pa, and the distillation time is 40 to 80 minutes; collecting distillate, and then performing a second grade distillation on the distillate, wherein the temperature of the evaporating surface is between 30 and 50 DEG C, the pressure is 60 to 80Pa, and the distillation time is 40 to 80 minutes; and then collecting the distillate, adding acetone, refrigerating, crystallizing, separating a crystal, washing and drying the crystal to obtain the product. The atractylon prepared by the method has high purity, and the industrial amplification is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation method of atractylone, especially a kind of preparation method who from plant, extracts atractylone.
Background technology
Atractylone (Atractylon) has another name called: atractyloxide, molecular formula: C
15H
20O, molecular weight: 216.322, CAS accession number: 6989-21-5, mainly there is feverfew Atractylis lancea Atractylodes lancea (Thunb.) DC., Atractylis chinensis Atractylodes chinensis (DC.) Koidz,, bighead atractylodes rhizome Atractylodes macrocephala Koidz. etc. in the various plants rhizome.Its molecular formula is as follows:
Modern study shows, atractylone have protect the liver, multiple pharmacologically active such as anti-oxidant, anti-inflammatory, antitumor, resisiting influenza virus.
In the prior art, relevant atractylone preparation technology's report seldom and usually is unfavorable for industrialization operation, and as having disclosed a kind of preparation method of atractylone among the Chinese patent literature CN100551366C: medicinal material adopts the silica gel column chromatography separation and purification after extracting, operate loaded down with trivial detailsly, be unfavorable for that industrialization amplifies.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, atractylone that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the dry rhizome that is selected from Atractylis lancea, Atractylis chinensis, the bighead atractylodes rhizome one kind of plant, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 1-4%, extracting pressure 30-60MPa, temperature 40-60 ℃, CO
2Flow 1-3ml/g crude drug min, extraction time 60-120min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 60-90 ℃, and pressure is 100-150Pa, distillation time 40-80min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 30-50 ℃, pressure is 60-80Pa, and distillation 40-80min collects overhead product, add acetone, the refrigeration crystallization, fractional crystallization washs, is drying to obtain.
CO
2The condition optimization of supercritical extraction is: the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 50MPa, 50 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 80min.
The 1st grade of molecule distillatory condition optimization is: the generating surface temperature is 80 ℃, and pressure is 120Pa, distillation time 60min.
The 2nd grade of molecule distillatory condition optimization is: the generating surface temperature is 40 ℃, and pressure is 70Pa, distillation 60min.
Adopt the present invention to prepare atractylone, be beneficial to big production operation, energy consumption is little, pollutes little.
The present invention is further elaborated below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get Atractylis lancea dry rhizome 10Kg, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 1%, extracting pressure 30MPa, 40 ℃ of temperature, CO
2Flow 10L/min, extraction time 60min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 60 ℃, and pressure is 100Pa, distillation time 40min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 30 ℃, pressure is 60Pa, and distillation 40min collects overhead product, add acetone, refrigeration crystallization, fractional crystallization, wash, be drying to obtain atractylone 22.5g, detect through HPLC, purity is 98.3%.
Embodiment 2
Get Atractylis lancea dry rhizome 10Kg, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 4%, extracting pressure 60MPa, 60 ℃ of temperature, CO
2Flow 30L/min, extraction time 120min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 90 ℃, and pressure is 150Pa, distillation time 80min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 50 ℃, pressure is 80Pa, and distillation 80min collects overhead product, add acetone, refrigeration crystallization, fractional crystallization, wash, be drying to obtain atractylone 25.5g, detect through HPLC, purity is 97.7%.
Embodiment 3
Get Atractylis lancea dry rhizome 10Kg, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 50MPa, 50 ℃ of temperature, CO
2Flow 20L/min, extraction time 80min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 80 ℃, and pressure is 120Pa, distillation time 60min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 40 ℃, pressure is 70Pa, and distillation 60min collects overhead product, add acetone, refrigeration crystallization, fractional crystallization, wash, be drying to obtain atractylone 23.8g, detect through HPLC, purity is 98.9%.
Embodiment 4
Get Atractylis chinensis dry rhizome 10Kg, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 50MPa, 50 ℃ of temperature, CO
2Flow 20L/min, extraction time 80min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 80 ℃, and pressure is 120Pa, distillation time 60min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 40 ℃, pressure is 70Pa, and distillation 60min collects overhead product, add acetone, refrigeration crystallization, fractional crystallization, wash, be drying to obtain atractylone 19.8g, detect through HPLC, purity is 98.6%.
Embodiment 5
Get bighead atractylodes rhizome dry rhizome 10Kg, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 50MPa, 50 ℃ of temperature, CO
2Flow 20L/min, extraction time 80min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 80 ℃, and pressure is 120Pa, distillation time 60min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 40 ℃, pressure is 70Pa, and distillation 60min collects overhead product, add acetone, refrigeration crystallization, fractional crystallization, wash, be drying to obtain atractylone 10.8g, detect through HPLC, purity is 99.1%.
Claims (4)
1. the preparation method of an atractylone is characterized in that described method is made up of the following step: get the dry rhizome that is selected from Atractylis lancea, Atractylis chinensis, the bighead atractylodes rhizome one kind of plant, pulverize, join CO
2In the supercritical extraction device, normal hexane is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 1-4%, extracting pressure 30-60MPa, temperature 40-60 ℃, CO
2Flow 1-3ml/g crude drug min, extraction time 60-120min gets extract, be injected into and carry out 2 grades of molecule distillations in the molecular still, wherein the 1st grade of distillatory generating surface temperature is 60-90 ℃, and pressure is 100-150Pa, distillation time 40-80min collects overhead product and carries out the 2nd grade of distillation, and the generating surface temperature is 30-50 ℃, pressure is 60-80Pa, and distillation 40-80min collects overhead product, add acetone, the refrigeration crystallization, fractional crystallization washs, is drying to obtain.
2. according to the preparation method of the described a kind of atractylone of claim 1, it is characterized in that described CO
2The condition of supercritical extraction is: the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 50MPa, 50 ℃ of temperature, CO
2Flow 2ml/g crude drug min, extraction time 80min.
3. according to the preparation method of the described a kind of atractylone of claim 1, it is characterized in that described the 1st grade of molecule distillatory condition is: the generating surface temperature is 80 ℃, and pressure is 120Pa, distillation time 60min.
4. according to the preparation method of the described a kind of atractylone of claim 1, it is characterized in that described the 2nd grade of molecule distillatory condition is: the generating surface temperature is 40 ℃, and pressure is 70Pa, distillation 60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010170570A CN101817806A (en) | 2010-05-13 | 2010-05-13 | Method for preparing atractylon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010170570A CN101817806A (en) | 2010-05-13 | 2010-05-13 | Method for preparing atractylon |
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|---|---|
| CN101817806A true CN101817806A (en) | 2010-09-01 |
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| CN201010170570A Pending CN101817806A (en) | 2010-05-13 | 2010-05-13 | Method for preparing atractylon |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010312A (en) * | 2010-11-09 | 2011-04-13 | 苏州派腾生物医药科技有限公司 | Preparation method for hypericin I |
| CN102058081A (en) * | 2010-11-22 | 2011-05-18 | 晨光生物科技集团股份有限公司 | Device for preparing black pepper oil resin |
| CN106955291A (en) * | 2017-04-11 | 2017-07-18 | 皮定业 | A kind of anti-inflammation medicament and preparation method thereof |
| CN108714117A (en) * | 2018-07-06 | 2018-10-30 | 山东煜煌信息咨询有限公司 | A kind of long-acting perfume and preparation method thereof |
| CN111377896A (en) * | 2020-03-03 | 2020-07-07 | 黑龙江中医药大学 | Compound separated from bighead atractylodes rhizome and having anti-tumor activity as well as preparation method and application thereof |
-
2010
- 2010-05-13 CN CN201010170570A patent/CN101817806A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010312A (en) * | 2010-11-09 | 2011-04-13 | 苏州派腾生物医药科技有限公司 | Preparation method for hypericin I |
| CN102058081A (en) * | 2010-11-22 | 2011-05-18 | 晨光生物科技集团股份有限公司 | Device for preparing black pepper oil resin |
| CN102058081B (en) * | 2010-11-22 | 2013-06-26 | 晨光生物科技集团股份有限公司 | Device for preparing black pepper oil resin |
| CN106955291A (en) * | 2017-04-11 | 2017-07-18 | 皮定业 | A kind of anti-inflammation medicament and preparation method thereof |
| CN106955291B (en) * | 2017-04-11 | 2018-08-07 | 重庆立见科技发展有限责任公司 | A kind of antibacterial anti-inflammatory medicament and preparation method thereof |
| CN108714117A (en) * | 2018-07-06 | 2018-10-30 | 山东煜煌信息咨询有限公司 | A kind of long-acting perfume and preparation method thereof |
| CN108714117B (en) * | 2018-07-06 | 2021-04-27 | 浙江丽芙秀化妆品有限公司 | Long-acting perfume and preparation method thereof |
| CN111377896A (en) * | 2020-03-03 | 2020-07-07 | 黑龙江中医药大学 | Compound separated from bighead atractylodes rhizome and having anti-tumor activity as well as preparation method and application thereof |
| CN111377896B (en) * | 2020-03-03 | 2021-08-20 | 黑龙江中医药大学 | Compound separated from bighead atractylodes rhizome and having anti-tumor activity as well as preparation method and application thereof |
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Application publication date: 20100901 |